Sodium sulfate decahydrate → tert-Butyl (3R)-3-(2-hydroxyethyl)piperidine-1-carboxylate

HRID 1761179노트

반응식

HRID 1761179 반응식
C([O:3][C:4](=O)[CH2:5][C@H:6]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7]1)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[OH:3][CH2:4][CH2:5][C@H:6]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7]1

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 29919087(R)-1-Boc-3-piperidine acetate ethyl ester

생성물 1

HCID 40425180tert-Butyl (3R)-3-(2-hydroxyethyl)piperidine-1-carboxylate수율 97.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 143 mg of t-butyl(3R)-3-(2-ethoxy-2-oxoethyl)tetrahydropyridine-1(2H)-carboxylate in 5 ml of tetrahydrofuran, 30 mg of litiumaluminum hydride was added under cooling with ice, followed by 20 minutes' stirring at the same temperature. To the reaction liquid sodium sulfate decahydrate was added, stirred for 12 hours and filtered with Celite. Distilling the solvent off under reduced pressure, 118 mg of the title compound was obtained.

후처리

  1. temperatureunder cooling with ice
  2. additionwas added
  3. stirringstirred for 12 hours
  4. filtrationfiltered with Celite
  5. distillationDistilling the solvent off under reduced pressure

출처 및 근거

ORD 기록
ord-1dd0d357d23e4e5585affb32963645e5
출처 데이터셋
uspto-grants-2005_01
특허 번호
US06846835B2

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